采用半微量高效液相色谱-电化学检测法测定大鼠血浆中曲格列酮立体异构体。

Determination of troglitazone stereoisomers in rat plasma using semi-micro HPLC with electrochemical detection.

作者信息

Suzuki Nobuyuki, Miyashita Naoto, Kotani Akira, Kusu Fumiyo, Kawasaki Takao

机构信息

Analytical and Quality Evaluation Research Laboratories, Sankyo Co. Ltd., 1-12-1, Shinomiya, Hiratsuka, Kanagawa 254-0014, Japan.

出版信息

J Pharm Biomed Anal. 2005 Jun 1;38(1):155-61. doi: 10.1016/j.jpba.2004.12.016.

DOI:10.1016/j.jpba.2004.12.016

PMID:15907634

Abstract

A highly sensitive determination method for troglitazone stereoisomers was developed by high-performance liquid chromatography with electrochemical detection (HPLC-ECD). The oxidation behavior of troglitazone was investigated for the application of ECD by measuring the cyclic voltammogram. The separation was performed on a semi-micro chiral column (Chiralcel OJ-RH) using a mobile phase consisting of methanol-acetic acid (1000:1, v/v) containing 50mM LiClO4 at a flow rate of 20 microl/min. The peak areas of the stereoisomers separated from 0.1 to 50 ng/ml of troglitazone had good linearity with correlation coefficients of >0.999, and had similar response. The limit of detection was 1.3 fmol (signal-to-noise ratio of 3). This method was applied to the determination of troglitazone stereoisomers in rat plasma. The levels of troglitazone stereoisomers in rat plasma could be monitored until 24h after the oral administration.

摘要

建立了一种采用高效液相色谱-电化学检测法（HPLC-ECD）测定曲格列酮立体异构体的高灵敏度方法。通过测量循环伏安图研究了曲格列酮的氧化行为，以应用于电化学检测。采用半微手性柱（Chiralcel OJ-RH）进行分离，流动相为含50mM高氯酸锂的甲醇-乙酸（1000:1，v/v），流速为20微升/分钟。从0.1至50 ng/ml曲格列酮中分离出的立体异构体的峰面积具有良好的线性，相关系数>0.999，且响应相似。检测限为1.3 fmol（信噪比为3）。该方法应用于大鼠血浆中曲格列酮立体异构体的测定。口服给药后24小时内可监测大鼠血浆中曲格列酮立体异构体的水平。